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#$Date: 2019-11-23 09:38:44 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232746 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/81/4348107.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4348107
loop_
_publ_author_name
'Hayne, David J.'
'White, Jonathan M.'
'McLean, Catriona A.'
'Villemagne, Victor L.'
'Barnham, Kevin J.'
'Donnelly, Paul S.'
_publ_section_title
;
 Synthesis of Oxorhenium(V) and Oxotechnetium(V) Complexes That Bind to
 Amyloid-β Plaques.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7944
_journal_page_last               7953
_journal_paper_doi               10.1021/acs.inorgchem.6b00972
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C15 H14 N3 O3 Re'
_chemical_formula_weight         470.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 100.626(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4901(4)
_cell_length_b                   8.0225(4)
_cell_length_c                   13.8963(4)
_cell_measurement_reflns_used    7184
_cell_measurement_temperature    130.0(1)
_cell_measurement_theta_max      34.2558
_cell_measurement_theta_min      2.9378
_cell_volume                     1368.56(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12472
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.362
_diffrn_reflns_theta_min         2.945
_exptl_absorpt_coefficient_mu    8.896
_exptl_absorpt_correction_T_max  0.298
_exptl_absorpt_correction_T_min  0.115
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.283
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.4797
_exptl_crystal_size_mid          0.2786
_exptl_crystal_size_min          0.1644
_refine_diff_density_max         1.578
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0.00263(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0212P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4654
_reflns_number_total             5347
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00972_si_001.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348107
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-1
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C4 C -0.2112(2) 0.7401(4) -0.1665(2) 0.0175(6) Uani 1 1 d . .
H4 H -0.2829 0.7743 -0.1873 0.021 Uiso 1 1 calc R U
C7 C 0.0072(2) 0.7954(3) 0.0597(2) 0.0156(5) Uani 1 1 d . .
H7A H -0.0153 0.9084 0.0708 0.019 Uiso 1 1 calc R U
H7B H -0.0212 0.7238 0.1053 0.019 Uiso 1 1 calc R U
C8 C 0.1634(2) 0.8227(4) 0.1884(2) 0.0156(5) Uani 1 1 d . .
H8A H 0.1268 0.7487 0.2270 0.019 Uiso 1 1 calc R U
H8B H 0.1457 0.9366 0.2030 0.019 Uiso 1 1 calc R U
C9 C 0.2864(3) 0.7966(4) 0.2152(2) 0.0185(6) Uani 1 1 d . .
H9A H 0.3242 0.9024 0.2171 0.022 Uiso 1 1 calc R U
H9B H 0.3055 0.7440 0.2789 0.022 Uiso 1 1 calc R U
C10 C 0.3898(2) 0.5633(4) 0.1620(2) 0.0151(5) Uani 1 1 d . .
C11 C 0.3926(2) 0.4545(3) 0.0747(2) 0.0143(5) Uani 1 1 d . .
C12 C 0.4641(2) 0.3215(4) 0.0772(2) 0.0178(6) Uani 1 1 d . .
H12 H 0.5128 0.2955 0.1343 0.021 Uiso 1 1 calc R U
C13 C 0.4615(3) 0.2286(4) -0.0070(3) 0.0179(6) Uani 1 1 d . .
H13 H 0.5106 0.1417 -0.0076 0.021 Uiso 1 1 calc R U
C14 C 0.3856(3) 0.2648(4) -0.0905(3) 0.0183(6) Uani 1 1 d . .
H14 H 0.3833 0.2027 -0.1474 0.022 Uiso 1 1 calc R U
C15 C 0.3130(2) 0.3955(3) -0.0878(2) 0.0155(5) Uani 1 1 d . .
H15 H 0.2602 0.4184 -0.1427 0.019 Uiso 1 1 calc R U
N1 N 0.1255(2) 0.7887(3) 0.08320(19) 0.0134(4) Uani 1 1 d . .
N2 N 0.3158(2) 0.6888(3) 0.13915(19) 0.0149(5) Uani 1 1 d . .
N3 N 0.31830(19) 0.4895(3) -0.00668(18) 0.0131(4) Uani 1 1 d . .
O1 O 0.27456(17) 0.8680(3) -0.05486(16) 0.0177(4) Uani 1 1 d . .
O2 O 0.10996(16) 0.5889(2) -0.08047(16) 0.0151(4) Uani 1 1 d . .
O4 O 0.44585(19) 0.5350(3) 0.24224(16) 0.0221(5) Uani 1 1 d . .
C1 C 0.0046(2) 0.6420(4) -0.1033(2) 0.0143(5) Uani 1 1 d . .
C2 C -0.0453(2) 0.7450(4) -0.0432(2) 0.0143(5) Uani 1 1 d . .
C3 C -0.1533(2) 0.7928(3) -0.0774(2) 0.0166(6) Uani 1 1 d . .
H3 H -0.1873 0.8625 -0.0387 0.020 Uiso 1 1 calc R U
C5 C -0.1618(2) 0.6358(4) -0.2249(2) 0.0172(5) Uani 1 1 d . .
H5 H -0.2003 0.5983 -0.2847 0.021 Uiso 1 1 calc R U
C6 C -0.0546(2) 0.5881(4) -0.1931(2) 0.0159(5) Uani 1 1 d . .
H6 H -0.0212 0.5187 -0.2324 0.019 Uiso 1 1 calc R U
Re1 Re 0.22678(2) 0.70965(2) 0.00636(2) 0.01107(4) Uani 1 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C3 C4 C5 119.6(3)
C3 C4 H4 120.2
C5 C4 H4 120.2
N1 C7 C2 116.6(2)
N1 C7 H7A 108.1
C2 C7 H7A 108.1
N1 C7 H7B 108.1
C2 C7 H7B 108.1
H7A C7 H7B 107.3
N1 C8 C9 109.9(2)
N1 C8 H8A 109.7
C9 C8 H8A 109.7
N1 C8 H8B 109.7
C9 C8 H8B 109.7
H8A C8 H8B 108.2
N2 C9 C8 106.3(2)
N2 C9 H9A 110.5
C8 C9 H9A 110.5
N2 C9 H9B 110.5
C8 C9 H9B 110.5
H9A C9 H9B 108.7
O4 C10 N2 126.7(3)
O4 C10 C11 122.3(3)
N2 C10 C11 110.9(3)
N3 C11 C12 121.3(3)
N3 C11 C10 116.1(2)
C12 C11 C10 122.5(3)
C13 C12 C11 118.6(3)
C13 C12 H12 120.7
C11 C12 H12 120.7
C12 C13 C14 120.1(3)
C12 C13 H13 119.9
C14 C13 H13 119.9
C13 C14 C15 118.9(3)
C13 C14 H14 120.6
C15 C14 H14 120.6
N3 C15 C14 120.8(3)
N3 C15 H15 119.6
C14 C15 H15 119.6
C7 N1 C8 110.0(2)
C7 N1 Re1 129.6(2)
C8 N1 Re1 119.38(18)
C10 N2 C9 121.2(3)
C10 N2 Re1 121.3(2)
C9 N2 Re1 116.81(19)
C15 N3 C11 120.2(2)
C15 N3 Re1 126.2(2)
C11 N3 Re1 113.39(19)
C1 O2 Re1 124.27(18)
O2 C1 C6 116.1(3)
O2 C1 C2 124.2(3)
C6 C1 C2 119.7(3)
C3 C2 C1 117.8(3)
C3 C2 C7 118.1(3)
C1 C2 C7 123.9(3)
C4 C3 C2 122.2(3)
C4 C3 H3 118.9
C2 C3 H3 118.9
C6 C5 C4 119.2(3)
C6 C5 H5 120.4
C4 C5 H5 120.4
C5 C6 C1 121.4(3)
C5 C6 H6 119.3
C1 C6 H6 119.3
O1 Re1 N1 111.24(10)
O1 Re1 O2 110.52(10)
N1 Re1 O2 90.79(9)
O1 Re1 N2 109.98(10)
N1 Re1 N2 79.78(10)
O2 Re1 N2 139.11(9)
O1 Re1 N3 109.52(9)
N1 Re1 N3 138.16(9)
O2 Re1 N3 83.60(9)
N2 Re1 N3 77.95(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C4 C3 1.380(5)
C4 C5 1.387(4)
C4 H4 0.9300
C7 N1 1.454(4)
C7 C2 1.514(4)
C7 H7A 0.9700
C7 H7B 0.9700
C8 N1 1.477(4)
C8 C9 1.526(4)
C8 H8A 0.9700
C8 H8B 0.9700
C9 N2 1.464(4)
C9 H9A 0.9700
C9 H9B 0.9700
C10 O4 1.224(3)
C10 N2 1.364(4)
C10 C11 1.500(4)
C11 N3 1.354(4)
C11 C12 1.388(4)
C12 C13 1.383(5)
C12 H12 0.9300
C13 C14 1.387(5)
C13 H13 0.9300
C14 C15 1.391(4)
C14 H14 0.9300
C15 N3 1.348(4)
C15 H15 0.9300
N1 Re1 1.908(2)
N2 Re1 1.978(3)
N3 Re1 2.130(2)
O1 Re1 1.697(2)
O2 C1 1.364(3)
O2 Re1 1.968(2)
C1 C6 1.396(4)
C1 C2 1.400(4)
C2 C3 1.399(4)
C3 H3 0.9300
C5 C6 1.385(4)
C5 H5 0.9300
C6 H6 0.9300
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 C8 C9 N2 -21.1(3)
O4 C10 C11 N3 173.2(3)
N2 C10 C11 N3 -4.8(3)
O4 C10 C11 C12 -4.6(4)
N2 C10 C11 C12 177.3(2)
N3 C11 C12 C13 2.7(4)
C10 C11 C12 C13 -179.6(3)
C11 C12 C13 C14 -2.5(4)
C12 C13 C14 C15 0.1(5)
C13 C14 C15 N3 2.2(4)
C2 C7 N1 C8 -173.6(2)
C2 C7 N1 Re1 -5.2(4)
C9 C8 N1 C7 173.7(2)
C9 C8 N1 Re1 3.9(3)
O4 C10 N2 C9 -7.1(5)
C11 C10 N2 C9 170.8(2)
O4 C10 N2 Re1 -177.0(2)
C11 C10 N2 Re1 0.9(3)
C8 C9 N2 C10 -139.1(3)
C8 C9 N2 Re1 31.2(3)
C14 C15 N3 C11 -2.0(4)
C14 C15 N3 Re1 172.8(2)
C12 C11 N3 C15 -0.5(4)
C10 C11 N3 C15 -178.3(2)
C12 C11 N3 Re1 -175.9(2)
C10 C11 N3 Re1 6.2(3)
Re1 O2 C1 C6 153.27(19)
Re1 O2 C1 C2 -26.6(4)
O2 C1 C2 C3 178.4(2)
C6 C1 C2 C3 -1.4(4)
O2 C1 C2 C7 -6.9(4)
C6 C1 C2 C7 173.3(3)
N1 C7 C2 C3 -162.4(2)
N1 C7 C2 C1 23.0(4)
C5 C4 C3 C2 0.2(4)
C1 C2 C3 C4 0.9(4)
C7 C2 C3 C4 -174.0(3)
C3 C4 C5 C6 -0.9(4)
C4 C5 C6 C1 0.4(4)
O2 C1 C6 C5 -179.1(2)
C2 C1 C6 C5 0.7(4)
